摘要
建立了乳制品中8种雌激素及6种孕激素残留的液相色谱-串联质谱(LC-MS/MS)同时测定方法。奶粉样品用水溶解后加甲醇提取(液态奶直接加甲醇提取),提取液加乙腈饱和正己烷除脂及亲水-亲脂平衡固相萃取柱净化后,采用ZORBAX Extend-C18色谱柱分离,分别在电喷雾正、负离子模式下以多反应监测(MRM)方式测定。正离子模式下的流动相为0.2%甲酸水溶液-乙腈,负离子模式下的流动相为0.1%氨水-乙腈。结果表明,14种激素在相应的浓度范围内相关系数均大于0.99,方法的平均回收率为61.6%～125.1%,相对标准偏差(RSDs)为1.9%～20%,检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.1～1.5μg/kg及0.3～5.0μg/kg。
A multi-residue method for the simultaneous determination of 8 estrogens and 6 progesterones in dairy by liquid chromatography-tandem mass spectrometry （LC-MS/MS） was developed. The powdered milk was dissolved in water, hormones were extracted with methanol （the analytes in liquid milk were extracted by methanol directly）, and the lipids in extract solution were removed by acetonitrile saturated n-hexane. The purification was carried out on a hydrophilic-lipophilic solid phase extraction column and separation was performed using a ZORBAX Extend-Cls column by gradient elution. Electrospray ionization mass spectrometry was operated in the positive or negative mode using multiple reaction monitoring（MRM） for the analytes. Acetonitrile and water with 0. 2% （V/V） formic acid were used as the mobile phase in the positive mode. Acetonitrile and water with 0. 1% （V/V） ammonia hydroxide were used as the mobile phase in the negative mode. The correlation coefficients of linear calibration curves were over 0. 99 in the corresponding concentration range. The average recoveries varied from 61.6% to 125. 1% , and the relative standard deviations（RSDs） were 1.9% -20%. The limits of detection （LOD, S/N = 3） and quantification （LOQ, S/N = 10） were 0. 1 -1.5 μg/kg and 0. 3 -5.0 μg/kg, respectively.
出处
《分析试验室》
CAS
CSCD
北大核心
2012年第11期76-81,共6页
Chinese Journal of Analysis Laboratory
关键词
液相色谱-串联质谱
固相萃取
雌激素
孕激素
液态奶
婴幼儿奶粉
乳
制品
Liquid chromatography-tandem mass spectrometry （ LC-MS/MS ）
Solid phase extraction （ SPE ）
Estrogens
Progesterones
Liquid milk
Infant formula
Dairy
